Process of making explosives.



No. 633,6. Patented Sept. 26, I899. F. G. & F. I. DU PDNT.

PROCESS OF MAKING EXPLOSIVES.

(Application filed Jan. 14, 1899/ (No Model.)

ATTORNEY WITNESSES: Mf/%W% ZQM m: 140mm mans 00., PNOYO-UITHE-v wunmcnou. Bic.

ilsrrnn STATES ATENT Fries.

FRANCIS G. DU PONT AND FRANCIS I. DU PONT, OF \VILMINGTON DELAWARE.

PROCESS OF MAKING EXPLOSIVES.

SPECIFICATION forming part of Letters Patent No. 633,611, dated September 26, 1899. Application filed Jan a 14, 1899. Serial No. 702,151. (No specimens.)

To all whom, it may concern.-

Be it known that we, FRANCIS G. DU PONT and FRANCIS LDU PONT, citizens of the United States, residing at Vilmington, in the county of New Castle and State of Delaware, have invented certain new and useful Improvements in the Manufacture of Explosives; and We do herebydeclare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same.

Ourinvention relates generally to the man ufacture of explosives, and particularly to improvements in processes of making smokeless explosives from nitro-glycerine and nitro-cellulose or gun-cotton.

The objects of our invention are to produce a smokeless explosive of high ballistic qualities, to avoid danger of explosion during the mixing of the gun-cotton and nitro-glycerine, and to render the manufacture of the explosive comparatively inexpensive. These objects are attained in the process herein described.

The process consists, in brief, in saturating gun-cotton with alcohol,dissolving nitro-glyccerinein ether, and then adding such solution to the alcoholized gun-cotton, thus causing the gun-cotton and nitro-glycerine to unite.

In the drawing which Y accompanies and forms a part of this specification we illustrate an apparatus which may be employed forsaturating gun-cotton uniformly with alcohol and displacing water in the gun-cotton preliminary to the mixture therewith of nitro-glycerine. This apparatus and the process of displacing the Water in the gun-cotton by means of alcohol are covered by Reissued Letters Patent No 11,651, dated February 15, 1898. The apparatus illustrated comprises a press (shown in section) and a series of liquidreceptacles and suitable piping.

In the drawing, M designates a press consisting of a cylinder N, provided with movable heads D and E, which may be moved longitudinally within the cylinder by means of screws DE, mounted within screw-thread ed hearings in bearing-plates D E, connected andsupportedbycolumnsO. Theinnerends of the cylinder-heads D and E are perforated, and within these heads are chambers d e ably of glass.

A, B, and O are measuring vessels, prefer- A pipe 1 connects the chamber (I of the press with a pipe 3,connected to the vessel 0 at the bottom. The chamber e is likewise connected to this pipe 3 through a pipe 14, pipe 3 being connected with pipes 1 and 14 by means of a suitable connectingpiece 2. The pipe 14 is also connected by means of the pipe '7, connecting-piece 8, and pipes 9 and 10 with vessels A and B, being connected with said vessels at the top. The vessels-A and B are connected at the top by a pipe 11, in which is a nipple 12, to which may be connected a pipe leading to an airpump. (Not shown.) In the pipe 14:, between the points of connection of the pipes 3 and '7 thereto, is a stop-cock a. In the pipes 9 and 10 are stop-cocks I) and d, respectively, and in the pipe 11 are cocks c and 6 upon opposite sides of the nipple 12.

In the carrying outof our process gun-cotton of the desired degree of nitration, preferably 1225 per cent., saturated with water, in which condition it is ordinarily kept to avoid danger of explosion, is placed within the cylinder N, the upper head D being removed for that purpose. Before placing the gun-cotton in the cylinder a layer of wire-cloth e is placed over the lower cylinder-head E, and after the gun-cotton has been placed in the cylinder and before the head D has been placed therein a similar layer of wire-cloth d is placed therein. The vessel 0, which occupies a somewhat higher elevation than the vessels A and B, is filled with alcohol. For convenience in carrying out the process it is preferable that this alcohol should be colored, and

for this purpose almost any dye soluble in alcohol may be used, although we prefer to use the dye called cudbear. The cocks a, d, e, andj and cooks h and t in the lower ends of vessels A and B are closed and the vacuumpump connected with the nipple 12 and operated. The suction thus produced will draw free liquid within the cylinderNinto the vessel A. \Vhen as much water as can be removed from the gun-cotton in this manner practicably has been so removed, pressure is applied by turning the screw D, so as to move the cylinder-head D downward and the cook a is opened, so that suction is applied at both ends of the cylinder. The water pressed from the gun-cotton is drawn into the vessel A. When this vessel becomes filled, the cocks b and 0 may be closed and the cooks (Z and opened, so that the water will be collected within the vessel B. The vessel A may then be emptied by opening the cock h and removiug the cork A. \Vhen as much water has been removed from the gun-cotton in this manner'as is practicable and when pressure sufficient to render the gun-cotton equally porous throughout has been applied, (and for this purpose we find that a pressure of from one hundred and fifty to two hundred pounds per square inch is sufficient,) the cock a is closed and the cockj opened, the air-pump still being kept in operation, cocks d and 6 being closed, if they have been opened, and in that case cocks b and 0 being opened. The alcohol from the vessel 0 now passes through the pipes 3 and 1 into the upper end of the cylinder and replaces the water in the guncotton, the water being drawn off by suction. After a' time, when the water has all been displaced, the color of the alcohol will be observed in the glass connection 6 in the pipe 14. at the point where the pipe 7 is connected thereto. The cocks Z) and c are then closed and the cooks (Z and e opened and the alcohol drawn into the vessel B, which, if it has contained fluid before, has been emptied preparatory to receiving the alcohol. The alcohol is drawn through the gun'cotton into the vessel B until ithas reached the strength of the alcohol in the vessel 0, which is shown by the color of the fluid in the pipe connections. The supply of alcohol is then cut off by closing the valve Pressure is applied by turning the screw D' to press out surplus alcohol, such surplus being drawn into vessel A by the action of the vacuum-pu mp. This process of replacing the Water in the gun-cotton by alcohol is termed percolation. By this operation all water has been removed from the gun-cotton, and it has been saturated with alcohol thoroughly and uniformly. It is then removed from the press,

placed within a mixer, such as is ordinarily employed to incorporate smokeless powder, and nitro-glycerine in solution in ether is added thereto in proper proportions. We prefer to employ a thirty-per-cent. solution of The mixer being nitro=glycerine in ether.

operated, the nitro-glycerinc is caused by the combined act-ion of the alcohol and ether to unite with the gun-cotton. This step of the process may be conducted without danger, as the nitro-glycerine when in solution in the ether is comparatively inexplosive. After the nitro-glycerine and gun-cotton have united the product is formed into the desired shape and the excess of solvent is allowed to evaporate.

WVe have found thatby saturating the guncotton with alcohol, as above described, and dissolving the nitro-glycerine in ether, and then adding such solution to the alcoholized gun-cotton, an intimate mixture of the nitroglycerine with the gun-cotton maybe obtained in less time than if the gun-cotton were dissolved in alcohol-ether and nitro-glycerine added to the solution, and a more powerful solvent is formed, so that a greater quantity of alcohol and less quantity of ether may be used. Inasmuch as during the entire operation the gun-cotton is moist, and since, as already stated, the addition of ether to the nitroglycerine avoids danger of explosion of the latter, the entire operation may be conducted without danger.

. Having thus completely described our i11- vention, What we claim, and desire to secure by Letters Patent, is

1. The herein-described process of making explosives, which consists in mixing alcohol with nitro-cellulose, and then mixing with the alcoholized nitro-cellulose a solution of nitro-glycerine in ether, substantially as de scribed.

2. The herein-described process of making explosives, which consists in displacing water in wet gun-cotton with alcohol by percolation, compressing the gun-cotton until only the desired quantity of alcohol remains therein, and mixing with the alcoholized gun-cotton a solution of nitro-glyeerine in ether, substantially as described.

In testimony whereof we hereunto affix our signatures in the presence of two witnesses.

FRANCIS G. DU PONT. FRANCIS I. DU PONT.

Witnesses:

J OHN W. MAoKLEM, EUSTIS W. GREEN. 

